CN102721758A - Method for measuring residues of pyrethroids pesticides in vegetables by gas chromatography - Google Patents
Method for measuring residues of pyrethroids pesticides in vegetables by gas chromatography Download PDFInfo
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- CN102721758A CN102721758A CN2012102039952A CN201210203995A CN102721758A CN 102721758 A CN102721758 A CN 102721758A CN 2012102039952 A CN2012102039952 A CN 2012102039952A CN 201210203995 A CN201210203995 A CN 201210203995A CN 102721758 A CN102721758 A CN 102721758A
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- pyrethrin pesticide
- chromatography determination
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Abstract
The invention discloses a method for measuring residues of pyrethroids pesticides in vegetables by gas chromatography. The method includes (1) extracting agent preparing; (2) extracting; (3) purifying; and (4) testing. The method for measuring residues of pyrethroids pesticides in vegetables by gas chromatography has the advantages of simplicity, convenience, feasibility, high quantitative recovery rate, low relative standard deviation and good stability.
Description
Technical field
The present invention relates to a kind of residual method of pyrethrin pesticide in the vegetables of measuring, be specifically related to a kind of residual method of pyrethrin pesticide in the gas chromatography determination vegetables that adopts.
Background technology
Pyrethrin pesticide is widely used for the vegetables deinsectization; People were once thinking once that such toxicity of pesticide was low, decomposition is fast, residual less, safe in utilization; But achievement in research in recent years shows that pyrethrin pesticide has cumulative toxicity, has developed into one of 3 types of main in vegetables, fruit remainss of pesticide, and there is serious threat in the words of long-term accumulated to health; So; Corresponding detecting method need be caught up with synchronously, does not also have the residual method of pyrethrin pesticide in a kind of simple and feasible mensuration vegetables at present, can satisfy the requirement that food safety supervision detects.
Summary of the invention
For solving the deficiency of prior art, the object of the present invention is to provide the residual method of pyrethrin pesticide in a kind of gas chromatography determination vegetables, simple and feasible, the quantitative recovery rate is high, good stability.
In order to realize above-mentioned target, the present invention adopts following technical scheme:
The residual method of pyrethrin pesticide is characterized in that in the gas chromatography determination vegetables, comprises the steps: that (1) preparation proposes agent: acetone and sherwood oil are mixed according to the volume ratio of 1:1, process the proposition agent, and for use; (2) extract: get vegetable sample and smash to pieces, with proposing the agent soaked overnight, vibrated then 30 minutes, standing demix is drawn upper strata stillness of night 5mL in the centrifuge tube of 5mL; (3) purify: make the test sample of treating in the centrifuge tube be about 3mL with the high pure nitrogen purging, purify through the Florish decontaminating column then, filtrate and continue purging near dried, be settled to 0.5mL with sherwood oil again with high pure nitrogen; (4) test: the gas chromatograph column temperature is remained on 65 ℃, and the retention time is 1 minute, rises to 280 ℃ with 20 ℃/minute then; Kept 25 minutes, the temperature of injection port is 280 ℃, and the temperature of electron capture organ is 300 ℃; Sample introduction 1 microlitre obtains the retention time of pyrethrin pesticide.
The residual method of pyrethrin pesticide is characterized in that in the aforesaid gas chromatography determination vegetables, and above-mentioned pyrethrin pesticide comprises cypermethrin, fenvalerate, decis.
The residual method of pyrethrin pesticide is characterized in that in the aforesaid gas chromatography determination vegetables, and above-mentioned gas chromatograph is the GC7890 gas chromatograph that carries electron capture organ.
The residual method of pyrethrin pesticide is characterized in that in the aforesaid gas chromatography determination vegetables, and the purity of above-mentioned high pure nitrogen is more than or equal to 99.999%.
Usefulness of the present invention is: the residual method of pyrethrin pesticide in the gas chromatography determination vegetables of the present invention, simple and feasible, the quantitative recovery rate is high, and relative standard deviation is less, good stability.
Description of drawings
Fig. 1 is the chromatogram of pyrethrin pesticide of the present invention.
Embodiment
Below in conjunction with accompanying drawing and specific embodiment the present invention is done concrete introduction.
The inventive method is applicable to cypermethrin, fenvalerate, the decis of measuring in the vegetables, comprises the steps:
(1) acetone and sherwood oil are mixed according to the volume ratio of 1:1, process the proposition agent, for use.Certainly, the acetone of this place's employing and sherwood oil are the gas chromatography level.
(2) extract: get vegetable sample and smash to pieces, with proposing the agent soaked overnight, vibrated then 30 minutes, standing demix is drawn upper strata stillness of night 5mL in the centrifuge tube of 5mL.In this step; Vegetable sample can be various vegetables such as green vegetables, cucumber, tomato; Be example with green vegetables in the present embodiment, its sampling quality does not have strict restriction, can earlier vegetables be cut into segment or fritter; And then with comminutor pulverizing or manual smashing to pieces, proposing agent is minimum use amount requirement with the submergence vegetable sample.
(3) purify: using purity is that 99.999% high pure nitrogen purges and makes the test sample of treating in the centrifuge tube be about 3mL, purifies through the Florish decontaminating column then, and filtrating is continued to purge near with high pure nitrogen and done, and is settled to 0.5mL with sherwood oil again.
(4) test: the GC7890 gas chromatograph column temperature that will carry electron capture organ remains on 65 ℃; Retention time is 1 minute, rises to 280 ℃ with 20 ℃/minute then, keeps 25 minutes; The temperature of injection port is 280 ℃; The temperature of electron capture organ is 300 ℃, and sample introduction 1 microlitre obtains the retention time of pyrethrin pesticide.
As can be seen from Figure 1: the cypermethrin retention time is the shortest, and the fenvalerate retention time is placed in the middle, and the decis retention time is the longest.Repeat this embodiment twice, note is made embodiment 1 and embodiment 2 respectively, obtain the yield as shown in table 1 and the recovery according to the external standard method area, and relative standard deviation is less.
The table 1 pyrethrin pesticide recovery and RSD table
More than show and described ultimate principle of the present invention, principal character and advantage.The technician of the industry should understand, and the foregoing description does not limit the present invention in any form, and all employings are equal to the technical scheme that mode obtained of replacement or equivalent transformation, all drop in protection scope of the present invention.
Claims (4)
1. the residual method of pyrethrin pesticide in the gas chromatography determination vegetables is characterized in that, comprises the steps: that (1) preparation proposes agent: acetone and sherwood oil are mixed according to the volume ratio of 1:1, process the proposition agent, and for use; (2) extract: get vegetable sample and smash to pieces, with proposing the agent soaked overnight, vibrated then 30 minutes, standing demix is drawn upper strata stillness of night 5mL in the centrifuge tube of 5mL; (3) purify: make the test sample of treating in the centrifuge tube be about 3mL with the high pure nitrogen purging, purify through the Florish decontaminating column then, filtrate and continue purging near dried, be settled to 0.5mL with sherwood oil again with high pure nitrogen; (4) test: the gas chromatograph column temperature is remained on 65 ℃, and the retention time is 1 minute, rises to 280 ℃ with 20 ℃/minute then; Kept 25 minutes, the temperature of injection port is 280 ℃, and the temperature of electron capture organ is 300 ℃; Sample introduction 1 microlitre obtains the retention time of pyrethrin pesticide.
2. the residual method of pyrethrin pesticide is characterized in that in the gas chromatography determination vegetables according to claim 1, and above-mentioned pyrethrin pesticide comprises cypermethrin, fenvalerate, decis.
3. the residual method of pyrethrin pesticide is characterized in that in the gas chromatography determination vegetables according to claim 1, and above-mentioned gas chromatograph is the GC7890 gas chromatograph that carries electron capture organ.
4. the residual method of pyrethrin pesticide is characterized in that in the gas chromatography determination vegetables according to claim 1, and the purity of above-mentioned high pure nitrogen is more than or equal to 99.999%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2012102039952A CN102721758A (en) | 2012-06-19 | 2012-06-19 | Method for measuring residues of pyrethroids pesticides in vegetables by gas chromatography |
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| CN2012102039952A CN102721758A (en) | 2012-06-19 | 2012-06-19 | Method for measuring residues of pyrethroids pesticides in vegetables by gas chromatography |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103454357A (en) * | 2013-09-13 | 2013-12-18 | 宁波新大昌织造有限公司 | Method for measuring effective components in mosquito repellent nets |
| CN103913528A (en) * | 2014-04-24 | 2014-07-09 | 江苏太湖地区农业科学研究所 | Quantitative detection method for pyrethriods pesticides in fresh tea |
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| JP2009053165A (en) * | 2007-08-29 | 2009-03-12 | Tsumura & Co | Method of purifying residual agricultural chemicals in herbal medicine sample |
| CN101915809A (en) * | 2010-07-01 | 2010-12-15 | 王冬群 | Detection method of pyrethroid pesticide remained in rice |
| CN102121928A (en) * | 2010-12-20 | 2011-07-13 | 天津市农业科学院中心实验室 | Method for processing onion sample containing several pesticide residues before determination |
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2012
- 2012-06-19 CN CN2012102039952A patent/CN102721758A/en active Pending
Patent Citations (3)
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| JP2009053165A (en) * | 2007-08-29 | 2009-03-12 | Tsumura & Co | Method of purifying residual agricultural chemicals in herbal medicine sample |
| CN101915809A (en) * | 2010-07-01 | 2010-12-15 | 王冬群 | Detection method of pyrethroid pesticide remained in rice |
| CN102121928A (en) * | 2010-12-20 | 2011-07-13 | 天津市农业科学院中心实验室 | Method for processing onion sample containing several pesticide residues before determination |
Non-Patent Citations (3)
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| 丁明等: "柿果和土壤中菊酯类农药的残留检测和消解动态研究", 《江西农业大学学报》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103454357A (en) * | 2013-09-13 | 2013-12-18 | 宁波新大昌织造有限公司 | Method for measuring effective components in mosquito repellent nets |
| CN103913528A (en) * | 2014-04-24 | 2014-07-09 | 江苏太湖地区农业科学研究所 | Quantitative detection method for pyrethriods pesticides in fresh tea |
| CN103913528B (en) * | 2014-04-24 | 2015-04-29 | 江苏太湖地区农业科学研究所 | Quantitative detection method for pyrethriods pesticides in fresh tea |
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Application publication date: 20121010 |